HRID1419226
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To 600 mg of 6-amidino-1-carbamoylmethyl-2-naphthyl 4-nitrobenzoate.hydrochloride were added 10 ml of anhydrous DMF and 100 mg of 10% palladium carbon, and catalytic reduction was effected at room temperature for 24 hours. Then, insoluble matter was filtered off and the filtrate was concentrated under reduced pressure. To the residue was added 15 ml of methanol, and, furthermore, 350 μl of concentrated hydrochloric acid was added with stirring under cooling with ice. Then, the resulting solution was added dropwise to 200 ml of acetone, followed by stirring for 1 hour under cooling with ice. Then, the precipitate was collected by filtration to obtain 572.7 mg of the desired product.
WORKUP
后处理
- filtrationThen, insoluble matter was filtered off
- concentrationthe filtrate was concentrated under reduced pressure
- additionTo the residue was added 15 ml of methanol
- additionfurthermore, 350 μl of concentrated hydrochloric acid was added
- temperatureunder cooling with ice
- additionThen, the resulting solution was added dropwise to 200 ml of acetone
- stirringby stirring for 1 hour
- temperatureunder cooling with ice
- filtrationThen, the precipitate was collected by filtration